関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Palmitic Acid | HCID 985 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 溶媒 | Cyclohexane | HCID 8078 | — |
| 生成物 | Palmitic anhydride | HCID 69339 | — |
反応手順
Palmitic acid (512.04 g, 2.00 moles) and acetic anhydride (204.05 g, 2.00 moles) were charged to a two liter reaction flask fitted with an overhead stirrer, thermometer, condenser and nitrogen inlet. The mixture was heated gently with stirring to allow the solid palmitic acid to melt (61° C. to 64° C.). Heating was continued until the reflux temperature had been reached (147° C.), this temperature was maintained for a period of one hour. The resultant mixture was cooled to room temperature to allow a light yellow solid to form, this was slurried in cyclohexane (100 ml), filtered and recrystallised from petroleum ether 60-80. The recrystallised wet solid was placed in a vacuum oven at 40° C. until dry of residual acetic acid. The resultant white powdery solid was stored under vacuum in the presence of silica gel. The yield of palmitic anhydride was 458.49 g which represented a 92.8% chemical yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05525709 |
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| 出典データセット | uspto-grants-1996_06 |
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| ORD ID | ord-dfd6bab83436493486bd1a795b68e9ad |
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| 出典メモ | uspto-grants-1996_06 |
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